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ISSN : 1225-0112(Print)
ISSN : 2288-4505(Online)
Applied Chemistry for Engineering Vol.12 No.6 pp.679-681
DOI :

Research Papers : Sol - Gel Synthesis of Reducing Agent of Silyl Ammonium Borohydride

Bo Hye Kim

Abstract

Silyl ammonium borohydride(SAB) was synthesized via acidic sol-gel route with subsequent cation exchange. The mole ratio of 1/1/4/2/1.0x10(-2) of 3-chloropropyl-triethoxy silane/dimethyldodecylamine/H2O/THF/HCl(catalyst) was determined to be the optimum for the sol-gel synthesis of silyl quarternary ammonium chloride(SAC). SAB was then prepared by the ionic metathesis of SAC and NaBH4. SAB was identified by the B-H stretching vibrations at 2371, 2320, 2274 cm(-1) on a FT-IR spectroscopy. The content of BH4(-) group in SAB was found to be 2.0 mmol/g. The gel SAC and SAB were found to have low surface area of amorphous structure and low thermal stability at high temperature, judged by TGA, BET, SEM, and low angle XRD analyses. The gel SAB was able to reduce PhCHO to PhCH2OH effectively.

연구논문 : Sol - Gel 법을 이용한 규소 - 보란 환원제의 합성

김보혜,우희권

초록

유기규소 사차 암모니움 보로하이드라이드(SAB)를 유기규소 사차 암모니움클로라이드(SAC)와 수소화붕소화나트륨으로 합성하였으며 유기규소 사차 암모니움클로라이드는 3-클로로프로필트리에톡시실란/디메틸도데실아민/물/테트라히드로푸란/염산(촉매)을 1/1/4/2/1.0x10(-2)의 몰비로 졸-겔 합성법에 따라 최적화 하였다. SAB의 합성은 FT-IR 스펙트럼의 2371,2320,2274 cm(-1)에서 새로운 B-H 신축 진동이 나타나는 것으로 확인하였으며 SAB1.0 g 당 BH4(-)의 함유량은 2.0 mmol이었다. 화합물 SAC와 SAB는 작은 표면적을 가지며 높은 온도에서 열안정성이 낮은 무정형의 겔상태구조임을 TGA, BET, SEM 그리고 XRD분석을 통하여 확인하였다. 겔상태의 화합물 SAB는 알데히드를 알코올로 환원시키는데 효과적이었다.

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